Treatment of lignocellulosic materials
This invention relates to a process for modifying lignocellulosic materials by a chemical treatment comprising treating the material sequentially or simultaneously with phthalic anhydride and a thermosetting resin at elevated temperature, and finally heat lignocellulosic material so produced can be formed into shapes or molds having excellent dimensional stability.
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The present invention relates to a process for modifying Lignocellulosic materials, especially wood e.g. in its shredded or particulate form to improve physical properties thereof.
It is well known in the art to modify wood by treating it with acetic acid and/or acetic anhydride in order to improve various physical properties of the wood such as the dimensional stability thereof. Such processes are claimed and described in a number of published patents such as e.g. EP-A-0 213 252, U.S. Pat. No. 2,417,995 and EP-A-0 063 160. It is also known to treat wood with phthalic anhydride to improve its physical properties. Such a method is reviewed in a book entitled "The Chemistry of Solid Wood" Ed by Rowell, R et al and published by the American Chemical Society, 1984 page 186. This book lists a number of references on page 208 including inter alia Popper, R et al in Holz Roh-Werkst.: 1972, 30(8), 289-94; 1973, 31(2), 65-70; and 1975, 33(11), 415-19.
These articles, however, point out that the effect of phthalic anhydride treatment is not long lasting and that the phthalic anhydride is hydrolysed and/or leached out from the wood when in contact with water.
It is also known from U.S. Pat. No. 2,140,981 and U.S. Pat. No. 4,486,475 to modify wood by impregnation with an aqueous solution of a thermosetting resin such as e.g. a phenol-formaldehyde resin. The problem with this method is that the wood so treated produces a product which does not have sufficient dimensional stability and water repellancy. Moreover, most of these use urea formaldehyde resins which are inferior to phenol-formaldehyde resins.
U.S. Reissue describes a process for treating preformed boards from wood type cellulosic material which are impregnated with phthalic annhydride and/or a thermosetting resin such as e.g. a phenolaldehyde resins.
It has now been found that such lignocellulosic materials can be treated with a combination of aromatic anhydrides and resins to obtain the relevant improvement in its properties prior to being formed into a board.
Accordingly, the present invention is a process for modifying lignocellulosic material (hereafter "LM") by a chemical treatment method, said method comprising treating the LM sequentially or simultaneously with:
a. phthalic anhydride and
b. a thermosetting resin, and
heat curing the phthalylated, resin-impregnated product so formed.
The LM to be treated can be any wood capable of being treated in the above manner including inter alia chips, flakes, splinters, strands, shreds, shives, fibres and which, after the treatment according to the invention, is capable of being shaped e.g. into a board, flat sheet, or other moulded product by shaping techniques well known in the art such as agglomeration using a suitable binding agent and one or more of heat, pressure, humidity, catalyst etc. The LM used is suitably wood which is preferably in the form of particles or shreds.
The treatment of the LM with phthalic anhydride and the thermosetting resin can be carried out sequentially or simultaneously. By this is meant that the wood may be treated with phthalic anhydride and the thermosetting resin in any sequence or by using a mixture of the two or by applying these two components simultaneously on to the LM. Each of the two components may be used as solid powders, individually as a solution in a solvent or as as solution of both in a single solvent. For instance, the phthalic anhydride (hereafter "PA") used is usually a solid and can be used in a form which enables uniform distribution over the LM being treated. Thus PA may be in the form of a powder, can be used in its molten form or as a solution or dispersion in a non-aqueous solvent but is is most preferably used in the form of a free flowing powder. Where it is used in the form of a powder, said powder suitably has an average particle size. The amount of PA used is suitably in the range from 1 to 50% w/w, preferably from 5 to 25% w/w based on the LM.
Where the treatment is carried out sequentially i.e. by treating the LM first with phthalic anhydride, the LM is suitably dried e.g. in an oven and then brought into contact with the PA by forming an intimate mixture of the two and the mixture is then cooked in a closed, suitably unsealed vessel at elevated temperature for a short duration. The drying process is carried out for a duration until there is no further loss of weight of the LM on extended drying. The desired degree of drying is usually achieved by drying for 1 hour at 105.degree. C.
The cooking process is suitably carried out at an elevated temperature which may be suitably at least 100.degree. C., preferably at least 140.degree. C. and more preferably in the range from 150.degree.-180.degree. C.
The cooking procedure may last from about 0.5 hr to about 5 hours depending upon the type of LM treated, the amount of PA used and the cooking temperature used. In any event, the cooking step should be carried out until the LM has a substantially constant weight.
Thereafter, the cooking is stopped and the contents of the vessel brought to ambient temperature. The above procedure is preferably conducted in such a manner that the LM has a weight gain of at least 15%, suitably at least 20% and preferably 25% upon completion of this step. The PA may optionally be combined with other known components such as insecticides, pesticides, perfumes or delivery systems used in the art for treating LM in step (a).
The resultant phthalylated product, optionally after an intervening cleaning step, is then impregnated with a thermosetting resin. Examples of such thermosetting resins include the phenolformaldehyde and urea-formaldehyde resins, urethane resins and the like. In the case of phenolic resins these are suitably resoles which are usually liquids but can be used in solid powder form, of, as a solution or dispersion thereof in a solvent. Examples of resins which can be used in the process of the present invention are sold under various trade names including the following:
BD 937 (ex Reichold, Canada is a phenol-aldehyde resin)
BD 804 (ex Reichold, Canada is a phenol-aldehyde resin)
BK 140 (ex Bakelite UK, is a phenol-aldehyde resin)
CELLOBOND.RTM. J2005A (ex BP Chemicals Ltd, an aqueous solution of a phenolic resole resin, solids content=65% w/w)
CELLOBOND.RTM. J2015A (ex BP Chemicals Ltd, a liquid phenol-formaldehyde resole resin, solids content=50% w/w)
CELLOBOND.RTM. J1047H (ex BP Chemicals Ltd, a phenol-formaldehyde Novolac resin ground with hexamine).
DDP 5064 (ex Dynochem, UK is a phenol-aldehyde resin).
R8821/1 (ex BP Chemicals Ltd, a solid phenol-formaldehyde resin).
These resins are the Novolac or resole type resins which are spray dried and, in some cases, are water soluble.
The impregnation with a thermosetting resin is suitably carried out by intimately mixing the LM (which may have been previously phthalylated in a sequential process as described above) with a resin in a finely divided powder form or in the form of a solution or a dispersion in a solvent. In the case of some resins, if used in powder form, it is preferable to initially dampen the phthalylated product with water, e.g. about 5-15% w/w, preferably 10% w/w, by thorough mixing. The dampened wood can then be mixed with the powdered resin and then transferred to a press to give the final board. One such resin CELLOBOND.RTM. J1047H (ex BP Chemicals Ltd, a phenol-aldehyde resin) which is used on a dampened phthalylated product.
The phthalylated, resin-impregnated product is heat cured suitably in such a manner that the core temperature of the treated LM is suitably >100.degree. C., preferably from 110.degree.-120.degree. C. This can be achieved by heating the phthalylated, resin-impregnated product suitably to a surface temperature of 150.degree.-250.degree. C., preferably from 170.degree.-220.degree. C.
Where the LM treated is wood in fibrous, particulate or shredded form, the resin-impregnated LM can be pressed in a die with a pre-heated punch to e.g. 5.5 mm stops at an elevated temperature of e.g. 180.degree. C. for a short duration e.g. 10 minutes. The resultant product can be in the shape of a board, flat sheet or a moulded product depending on the shape of the die and the pressure applied. Boards etc. produced from such LMs can be conditioned at a desired relative humidity (hereafter "RH") e.g. 65% and at a temperature of about 20.degree. C. before testing for its physical characteristics.
Where the treatment of the LM is carried out either simultaneously,or, in a reverse sequence to that described above, i.e. initially with a thermosetting resin and then with phthalic anhydride, the cooking of the phthalylated LM at elevated temperature can be omitted and the phthalylated, resin-impregnated LM can be subjected directly to heat curing as described above.
The boards thus produced from particles of LM were tested under static bending conditions and after soaking in water for 24 hours. The boards were also tested for internal bond strength and swelling after soaking in cold and hot water respectively.
The above tests showed that the boards thus produced had high dimensional stability and excellent resistance to water and to swelling when exposed to water. Moreover, the phthalic anhydride applied to the LM did not leach out from the LM upon soaking or exposure to water to any significant extent.
The present invention is further illustrated with reference to the following Examples.
EXAMPLESThe LM to be modified comprised a mixture of shreds from hardwoods and softwoods (50/50 w/w, particle size 2 mm.times.0.15 mm). The LM was first oven-dried then mixed with various amounts of powdered phthalic anhydride as shown in the Table below. The mixture was cooked in a closed, but not sealed, container at 160.degree. C. for 1 hour. The product was not cleaned prior to use. The modified LM product corresponded to the weight gain equivalent of the amount of the chemicals used.
The crude PA modified LM was dampened with 10% w/w water, stirred in with a food mixer, and then 10% w/w of powdered resin added thereto and mixed in. In the case where a liquid resin such as CELLOBOND.RTM. J2005A was used, it was diluted to 50% w/w solids and added to the PA modified LM. The resinated mixture was then pressed in a die with a pre-heated punch to 5.5 mm stops at 180.degree. C. for 10 minutes to form the boards. The boards so formed were conditioned no 65% relative humidity at 20.degree. C. before testing.
The conditioned boards as such and after soaking in water at 20.degree. C. for 24 hours, were tested under static bending using the method of BS1142/90 as a guide. A sample of this board was tested for internal bond strength and another sample of the board was measured for swelling after
a) a soaking in water at 20.degree. C. for 24 hours;
b) after 2 hour boil and 1 hour cold soak; and
c) after drying at 70.degree. C. followed by reconditioning at 20.degree. C. and 65% relative humidity to constant weight.
These samples were then tested for internal bond strength using the method of BS5669.
The procedure used for making the boards and the results are tabulated below:
TABLE 1
______________________________________
Formulation
used in Ingredients Adhesive
______________________________________
CT 1 Unmodified shred +10% BD 937
Example 1
5% phthalylated shred
+10% BD 937
Example 2
17.5% phthalylated shred
+10% BD 937
Example 3
25% phthalylated shred
+10 BD 937
CT 2 unmodified shred +10% J2005A solids
Example 4
10% phthalylated shred
+10% J2005A solids
Example 5
17.5% phthalylated shred
+10% J2005A solids
Example 6
25% phthalylated shred
+10% J2005A solids
CT 3 unmodified shred +10% DDP 5064
Example 7
17.5% phthalylated
+10% DDP 5064
Example 8
25% phthalylated shred
+10% DDP 5064
*CT 4 unmodified shred +10% BD 804
Example 9
10% phthalylated shred
+10% BD 804
Example 10
25% phthalylated shred
+10% BD 804
CT 5 unmodified shred +10% R8821/1
Example 11
17.5% phthalylated shred
+10% R8821/1
______________________________________
CT Comparative Test not according to the invention.
TABLE 2
__________________________________________________________________________
Results of static bending tests, given as conventional moduli.
Dry Static Bending
Wet Static Bending
Retained properties
Density
MOR MOE WTF/Vol
MOR MOE WTF/Vol
MOR MOE WTF/Vol
Name Kg/m.sup.3
MPa MPa kPa MPa MPa kPa % % %
__________________________________________________________________________
CT 1 1021 25.0
2846
15.6 8.9
861
7.8 36 30 50
Example 1
924 26.1
2896
19.5 21.6
1891
22.4 83 65 115
Example 2
949 29.1
3783
14.6 21.1
1991
20.8 73 53 142
Example 3
869 28.6
3764
12.2 29.9
2009
30.3 105 53 248
CT 2 978 39.8
4441
21.8 35.3
2140
44.9 89 48 206
Example 4
961 44.4
4559
26.3 26.5
2527
22.0 60 55 84
Example 5
957 35.2
4485
17.0 22.8
2542
17.7 65 57 104
Example 6
900 37 3616
24.3 29.1
2005
34.4 79 55 142
CT 3 999 28 2979
17.4 8.1
752
7.1 29 25 41
Example 7
975 32.5
4187
16.0 16.2
1597
14.0 50 38 88
Example 8
978 27.2
3665
12 14.1
1116
15.4 52 30 128
CT 4 970 17.3
2251
9.2 4.4
435
3.4 25 19 37
Example 9
952 23.2
3752
10.3 11.7
1181
10.3 51 31 100
Example 10
915 29.7
3178
18.3 16.1
1359
16.4 54 43 90
CT 9 1003 36.8
4383
24.8 10.7
1228
10.9 29 28 44
Example 11
926 25.6
3637
12.0 14.6
1651
11.5 57 45 95
__________________________________________________________________________
MOE Modulus of Elasticity
WTF Work to Failure
MOR Modulus of Rupture
CT Comparative Tests not according to the invention
TABLE 3
__________________________________________________________________________
Internal Bond Strength (IBS) and Swelling Data
Original
Boiled Cold Soak
2 hour boil
Reconditioned
Linear
Density
IBS IBS Retained
weight
swell
weight
swell
Weight
swell
swell
Name Kg/m.sup.3
kPa kPa % gain %
% gain %
% gain %
% %
__________________________________________________________________________
CT 1 1021 2107 276
13 30 14 64 33 0 17
Example 1
1054 3894 2507
64 21 9 46 24 1.7 13 0
Example 2
997 4300 2445
57 25 9 44 21 -0.4 8 -0.2
Example 3
869 4617 2712
59 20 5 53 11 4 1
CT 2 978 6029 700
12 21 8 65 37 1 21
Example 4
969 3811 4503
118 11 4 38 17 2 7 -0.3
Example 5
937 3389 4292
127 12 3 41 13 0.7 4 -0.1
Example 6
900 4674 3685
79 15 4 47 11 4 3
CT 3 999 1634 212
13 32 13 75 41 0 29
Example 7
964 1990 2905
146 16 6 39 17 0.4 7 -0.3
Example 8
978 2910 2000
69 15 3 39 10 1 0
CT 4 970 1041 291
28 42 22 104 68 2 40
Example 9
1007 2817 707
25 31 15 55 29 -0.1 17 0.1
Example 10
915 2935 1711
58 28 6 50 13 3 3
CT 5 1052 3390 542
16 22 10 59 38 2.4 21 0.2
Example 11
932 3438 1520
44 25 8 49 25 0 11 0.1
__________________________________________________________________________
EXAMPLES
These Examples were carried out to test the performance of boards prepared from shreds treated by the single-step simultaneous treatment thereof with a mixture of phthalic anhydride and the resin.
As in the above Examples a further wood substrate was prepared by mixing shreds (2 mm.times.0.15 mm) of hardwoods and softwoods (50/50). The resin used was CELLOBOND.RTM. J2015A, a phenolic resin ex BP Chemicals Ltd.
In this case, a known weight of phthalic anhydride was mixed into a stirred solution of the resin to give a homogeneous solution/dispersion and this is referred to as a `modified resin`.
The quantities of phthalic anhydride used to produce this preliminary modified resin were 5%, 10% and 17.5% w/w based on the dry wood. This phthalic anhydride was mixed into a sample of the resin equivalent to 10% w/w of the dry wood. The ratio of phthalic anhydride to resin in this modified resin was therefore:
______________________________________
phthalic anhydride (w/w)
J2015A Resin (w/w)
______________________________________
50 100
100 100
175 100
______________________________________
The wood to be used was oven dried and thereafter the modified resin was added thereto. The resinated mixture was then pressed in a die with a pre-heated punch at 5.5 mm stops at 180.degree. C. for 10 minutes to produce completed boards. These completed boards were then conditioned to 65% relative humidity at 20.degree. C. before testing.
The boards were tested under static bending, both conditioned and after a 24 hour 20.degree. C. water soak, using the method of BS1142/90 as a guide. A sample was tested for internal bond strength using the method of BS5669. Another sample was measured for swell after (i) the water soak treatment; (ii) after 2 hour boil and 1 hour cold soak; and after drying at 70.degree. C. followed by reconditioning as described in the Examples above. This sample was then tested for internal bond strength also.
TABLE 4
______________________________________
The procedure of simultaneous addition of phthalic anhydride and
the resin and results. The results achieved are tabulated below:
Formulation
used in Procedure Adhesive %
______________________________________
CT 6 Normal shred with 10% J 2015A
0 + 10
resin, 10 min 180.degree. C.
Example 12
Normal shred with 5% phthalic
5 + 10
anhydride and 10% J2015A resin,
10 min 180.degree. C.
Example 13
Normal shred with 10% phthalic
10 + 10
anhydride and 10% J2015A resin,
10 min 180.degree. C.
Example 14
Normal shred with 17.5% phtalic
17.5 + 10
anhydride and 10% J2015A resin,
10 min 180.degree. C.
______________________________________
TABLE 5
__________________________________________________________________________
Results of static bending tests on boards made by simultaneous addition,
given as conventional moduli.
Dry Static Bending
Wet Static Bending
Retained properties
Density
MOR MOE WTF/Vol
MOR MOE WTF/Vol
MOR MOE WTF/Vol
Name Kg/m.sup.3
MPa MPa kPa MPa MPa kPa % % %
__________________________________________________________________________
CT 6 944 26.9
3338
15.1 9.1
878
7.7 34 26 51
Example 12
1006 44.9
4745
25.6 25.7
1822
33.1 57 38 130
Example 13
951 36.7
3771
23.2 24.5
2084
26.8 67 55 116
Example 14
945 33.9
4091
17.4 25.3
1824
37.7 75 45 216
__________________________________________________________________________
MOE Modulus of Elasticity
WTF Work to Failure
MOR Modulus of Rupture
CT Comparative Tests not according to the invention
TABLE 6
__________________________________________________________________________
Internal Bond Strength and Swelling Data
Original
Boiled Cold Soak
2 hour boil
Reconditioned
Linear
Density
IBS IBS Retained
weight
swell
weight
swell
weight
swell
swell
Name Kg/m.sup.3
kPa kPa % gain %
% gain %
% gain %
% %
__________________________________________________________________________
CT 6 921 1873 624
33 17 9 64 46 2 27 0.2
Example 12
1017 5406 2086
39 13 7 49 28 1 14 0.1
Example 13
1005 6076 1897
31 15 11 53 30 0 14 0.1
Example 14
990 6458 1610
25 13 7 49 23 -1 11 -0.3
__________________________________________________________________________
The above results show that using the single step process, even by using
the phthalic anhydride and resin at the lowest level, boards were obtaine
which were stronger, stiffer and tougher and these boards also had a
higher internal bond strength than the unmodified control boards or board
modified with phthalic anhydride alone.
The above Examples and comparative tests were carried out using boards which were somewhat smaller in their dimensions than is recommended by the British Standard tests (BS 5669). In order to test the improvement in performance further, the following additional Examples and tests were carried out with boards which were increased in scale so as to meet fully the specification of BS 5669 tests. Two methods were used in the following Examples and tests.
In the first method, referred to here as the modification method, the wood shred was made by mixing oven-dry softwood shred with a measured quantity of finely ground PA and heated in an oven at 160.degree. C. for a period of 1 hr. This shred was stirred with CELLOBOND.RTM. J2005A liquid phenolic resin (5% wt/wt solids as a 50% solution) for 1 minute. A mattress was then formed and pressed at 170.degree. C. for 12 minutes, including closing time to form the board. A slow pressure release was then used.
In the second method, referred to here as the addition method (and in which the sequence of addition of PA and thermosetting resin was reversed), unmodified wood shred was stirred with J2005A liquid phenolic resin (5% wt/wt solids, as a 50% solution) for 30 seconds. The required quantity of finely ground PA was then added and stirred in for a further 30 seconds. The board was then made by pressing at 170.degree. C. as described in the first method above.
Four boards of each type were produced.
The physical testing of the boards was carried out as follows:
The boards were allowed to stabilise for 5 minutes after pressing, to allow for any variation or changes in dimensions that may occur during the initial stages immediately after formation. The thickness of each board was then measured at four marked positions about 5 cm in from the centre of each edge. A line was drawn on the board and two marks about 25 cm apart were made across the line. The distance between the marks was measured with a ruler.
The boards were then conditioned at 65% relative humidity (r.h.) and 20.degree. C. The thickness at the marked positions and the distance between the two marks were then measured again. The boards were marked out and cut into samples as shown in the sketch (not to scale) below:
______________________________________
F C
A G J K B
H
I D
______________________________________
Sample A--used for static bending testing at 65% r.h.
Sample B--used for static bending testing after soaking in water at 20.degree. C. for 24 hrs.
Sample C--used to measure thickness and linear swell and water uptake on soaking in water for 1 hr and 42 hrs.
Sample D--used to measure thickness and linear swell and water uptake on conditioning to 93% r.h. and 20.degree. C., and after boiling in water for 2 hrs (DIN 100).
Samples E,F,H and I--one each of each type of board for IBS testing after:
--conditioning at 93% r.h. and 20.degree. C.
--1 hour water soak at 20.degree. C.
--24 hour water soak at 20.degree. C.
--2 hour boil (DIN 100).
Sample J--used for V313 cyclical testing.
Sample K--used for non-standard cyclical testing.
The non-standard cyclical testing procedure used was as follows: The samples were weighed and measured for thickness, width and length. They were then oven-dried at 105.degree. C. and weighed and measured for thickness. The samples were then boiled in water for 2 hours, followed by drying at 105.degree. C. for about 20 hrs. This was followed by weighing and thickness measurement. The boiling, drying and measurement cycles were repeated for five cycles. The samples were then conditioned at 65% r.h. and 20.degree. C. before being weighed and measured for thickness, width and length. Finally, the IBS of the samples was measured.
The following calculations were applied to the results obtained:
A. Static Bending Tests
Two sets of calculations were carried out on the results of the stating bending tests. The conventional modulus of rupture (MOR), modulus of elasticity (MOE) were calculated according to BS 5669. The work to failure per unit volume (WTF/vol) was also calculated.
B. Internal Bond Strength (IBS)
In measuring the strength of the wood/matrix bond, effectively, a short, fat chain is being snapped. The chain will break at its weakest link. For quality control work, the existence of such weak links is of great commercial significance.
C. Other Results
Swelling, linear expansion and water uptake have been calculated as in BS 5669.
The results from all the above additional Examples and tests are tabulated below:
TABLE 7
__________________________________________________________________________
Results of static bending tests at relative humidity 65%
Ex. Conditioned 24 hour soak Retention
Ref MOR MOE WTF/Vol
MOR MOE WFT/Vol
MOR MOE WTF/V
No. Type MPa MPa kPa MPa MPa kPa % % %
__________________________________________________________________________
FZ 3
control
24.2
4086
13.1 9.5
1033
9.0 39 25 69
FZ 4
control
23.6
3919
12.5 7.2
877
5.5 30 22 44
FZ 5
control
20.8
4047
8.1 7.1
831
6.9 34 21 85
FZ 6
control
19.9
3799
9.1 5.5
562
4.5 28 15 49
mean 22.1
3963
10.7 7.3
826
6.5 33 21 62
FZ 12
10% mod.
26.7
4173
12.6 14.8
1545
15.3 56 37 121
FZ 13
10% mod.
28.1
4077
13.2 19.5
1750
17.7 69 43 134
FZ 14
10% mod.
31.4
4620
14.0 17.9
1880
12.0 57 41 86
FZ 15
10% mod.
31.4
4554
14.3 20.2
2138
17.4 64 47 122
mean 29.4
4356
13.5 18.1
1828
15.6 62 42 116
FY 87
14% mod.
35.4
5060
16.4 20.9
2477
15.2 59 49 93
FY 88
14% mod.
31.1
4966
12.5 28.7
3384
15.9 92 68 127
FY 89
14% mod.
26.2
4826
9.5 21.4
2147
16.9 82 44 178
FY 90
14% mod.
31.5
5046
13.1 22.9
2722
13.9 73 54 106
mean 31.1
4974
12.9 23.5
2682
15.5 76 54 126
FY 93
18% mod.
36.9
6329
13.1 24.1
2994
13.5 65 47 103
FY 94
18% mod.
29.6
5496
9.9 23.9
2771
14.5 81 50 146
FY 95
18% mod.
31.3
5157
11.6 28.7
3376
17.0 92 65 146
FY 96
18% mod.
33.0
5756
12.1 22.8
2584
14.9 69 45 123
mean 32.7
5685
11.7 24.9
2931
14.9 77 52 129
FZ 23
10% add.
28.9
5189
10.5 26.4
3594
13.2 91 69 125
FZ 24
10% add.
34.5
5440
14.1 26.3
3071
16.9 76 56 120
FZ 25
10% add.
34.0
5713
13.3 27.1
3466
14.5 80 61 109
FZ 26
10% add.
30.4
4924
12.1 30.1
3119
19.5 99 63 162
mean 31.9
5317
12.5 27.5
3312
16.0 87 62 129
FZ 33
14% add.
30.9
5786
10.2 26.1
2541
15.5 85 44 151
FZ 34
14% add.
32.2
5776
11.5 28.1
3617
14.0 87 63 122
FZ 35
14% add.
32.4
5909
11.2 29.2
3756
15.6 90 64 139
FZ 36
14% add.
27.7
4922
9.9 25.5
3551
13.0 92 72 131
mean 30.8
5598
10.7 27.2
3366
14.5 89 61 136
FZ 43
18% add.
29.0
5696
9.1 29.0
4349
12.1 100 76 134
FZ 44
18% add.
32.3
5994
11.1 26.3
3541
13.4 81 59 121
FZ 45
18% add.
33.1
5833
11.7 31.1
4186
14.9 94 72 127
FZ 46
18% add.
30.2
4976
11.4 33.3
4420
16.0 110 89 141
mean 31.2
5624
10.8 29.9
4124
14.1 96 74 131
__________________________________________________________________________
TABLE 8
______________________________________
Internal bond strength - 93% relative humidity
Board 65% r.h. 93% r.h.
from Ex density IBS density
IBS retention
Ref No. Type Kg/m.sup.3
kPa Kg/m.sup.3
kPa %
______________________________________
FZ 3 control 1008 1564 966 1100
FZ 4 control 1005 1722 1019 1318
FZ 5 control 1053 2353 1036 1655
FZ 6 control 990 1855 970 915
weighted 1014 1977 998 1358 69
mean
FZ 12 10% mod. 1005 3677 965 2670
FZ 13 10% mod. 995 3573 990 3147
FZ 14 10% mod. 980 3733 931 2705
FZ 15 10% mod. 978 3620 958 2916
weighted 990 3677 961 2923 79
mean
FY 87 14% mod. 984 3143 1010 2870
FY 88 14% mod. 996 3358 961 3170
FY 89 14% mod. 1001 3431 977 3007
FY 90 14% mod. 1044 3980 1022 2610
weighted 1006 3590 992 3015 84
mean
FY 93 18% mod. 1008 3973 926 2800
FY 94 18% mod. 1030 4050 1034 3649
FY 95 18% mod. 1025 3955 1032 3356
FY 96 18% mod. 1042 3903 991 3632
weighted 1026 3993 996 3546 89
mean
FZ 23 10% add. 961 2872 997 2170
FZ 24 10% add. 980 3338 966 2040
FZ 25 10% add. 993 3056 999 2146
FZ 26 10% add. 986 3070 988 2111
weighted 980 3155 988 2143 68
mean
FZ 33 14% add. 956 3337 987 2100
FZ 34 14% add. 983 3821 951 0
FZ 35 14% add. 987 3596 955 2161
FZ 36 14% add. 873 2664 882 1920
weighted 950 3584 944 2060 57
mean
FZ 43 18% add. 947 3463 979 2787
FZ 44 18% add. 962 3460 976 2730
FZ 45 18% add. 994 4109 941 2496
FZ 46 18% add. 915 3298 943 0
weighted 955 3677 960 2671 73
mean
______________________________________
TABLE 9
______________________________________
Internal bond strength - 1 hour cold soak
1 hour
Board 65% r.h. cold soak
from Ex density IBS density
IBS retention
Ref No. Type Kg/m.sup.3
kPa Kg/m.sup.3
kPa %
______________________________________
FZ 3 control 1008 1564 1016 1888
FZ 4 control 1005 1722 977 1270
FZ 5 control 1053 2353 973 1417
FZ 6 control 990 1855 962 648
weighted 1014 1977 982 1525 77
mean
FZ 12 10% mod. 1005 3677 999 3296
FZ 13 10% mod. 995 3573 973 3561
FZ 14 10% mod. 980 3733 921 3014
FZ 15 10% mod. 978 3620 972 3422
weighted 990 3677 966 3426 93
mean
FY 87 14% mod. 984 3143 995 3774
FY 88 14% mod. 996 3358 1006 3863
FY 89 14% mod. 1001 3431 983 3594
FY 90 14% mod. 1044 3980 1007 4004
weighted 1006 3590 998 3880 108
mean
FY 93 18% mod. 1008 3973 956 3407
FY 94 18% mod. 1030 4050 1015 3742
FY 95 18% mod. 1025 3955 987 4061
FY 96 18% mod. 1042 3903 1012 4014
weighted 1026 3993 992 3939 99
mean
FZ 23 10% add. 961 2872 1009 3340
FZ 24 10% add. 980 3338 1046 3670
FZ 25 10% add. 993 3056 982 3035
FZ 26 10% add. 986 3070 1000 3311
weighted 980 3155 1009 3440 109
mean
FZ 33 14% add. 956 3337 995 3387
FZ 34 14% add. 983 3821 1051 4021
FZ 35 14% add. 987 3596 967 3171
FZ 36 14% add. 873 2664 1013 4021
weighted 950 3584 1006 3810 106
mean
FZ 43 18% add. 947 3463 985 3893
FZ 44 18% add. 962 3460 952 3522
FZ 45 18% add. 994 4109 948 3465
FZ 46 18% add. 915 3298 932 3237
weighted 955 3677 954 3627 99
mean
______________________________________
TABLE 10
______________________________________
Internal bond strength - 24 hour cold soak
24 hour
Board 65% r.h. cold soak
from Ex density IBS density
IBS retention
Ref No. Type Kg/m.sup.3
kPa Kg/m.sup.3
kPa %
______________________________________
FZ 3 control 1008 1564 948 776
FZ 4 control 1005 1722 946 236
FZ 5 control 1053 2353 1035 520
FZ 6 control 990 1855 985 503
weighted 1014 1977 979 600 30
mean
FZ 12 10% mod. 1005 3677 979 3072
FZ 13 10% mod. 995 3573 935 2969
FZ 14 10% mod. 980 3733 973 3020
FZ 15 10% mod. 978 3620 965 3107
weighted 990 3677 963 3067 83
mean
FY 87 14% mod. 984 3143 966 3329
FY 88 14% mod. 996 3358 1020 3786
FY 89 14% mod. 1001 3431 926 2928
FY 90 14% mod. 1044 3980 1018 3573
weighted 1006 3590 982 3563 99
mean
FY 93 18% mod. 1008 3973 1010 3615
FY 94 18% mod. 1030 4050 978 3320
FY 95 18% mod. 1025 3955 996 3515
FY 96 18% mod. 1042 3903 1043 4091
weighted 1026 3993 1007 3740 94
mean
FZ 23 10% add. 961 2872 921 2067
FZ 24 10% add. 980 3338 1019 2877
FZ 25 10% add. 993 3056 989 2246
FZ 26 10% add. 986 3070 1016 2677
weighted 980 3155 986 2600 82
mean
FZ 33 14% add. 956 3337 962 2769
FZ 34 14% add. 983 3821 993 3484
FZ 35 14% add. 987 3596 1001 2830
FZ 36 14% add. 873 2664 956 2787
weighted 950 3584 978 3034 85
mean
FZ 43 18% add. 947 3463 959 2806
FZ 44 18% add. 962 3460 902 2837
FZ 45 18% add. 994 4109 968 2723
FZ 46 18% add. 915 3298 924 2857
weighted 955 3677 938 2833 77
mean
______________________________________
TABLE 11
______________________________________
Internal bond strength - DIN 100
Board from 65% r.h. DIN 100
Ex Ref density IBS density
IBS retention
No. Type Kg/m.sup.3
kPa Kg/m.sup.3
kPa %
______________________________________
FZ 3 control 1008 1564 953 103
FZ 4 control 1005 1722 2349 75
FZ 5 control 1053 2353 1065 477
FZ 6 control 990 1855 974 157
weighted 1014 1977 1335 245 12
mean
FZ 12 10% mod. 1005 3677 921 1980
FZ 13 10% mod. 995 3573 974 2652
FZ 14 10% mod. 980 3733 981 2559
FZ 15 10% mod. 978 3620 983 2332
weighted 990 3677 965 2514 68
mean
FY 87 14% mod. 984 3143 950 2725
FY 88 14% mod. 996 3358 948 2510
FY 89 14% mod. 1001 3431 986 2804
FY 90 14% mod. 1044 3980 1023 3179
weighted 1006 3590 977 2903 81
mean
FY 93 18% mod. 1008 3973 973 25,-5
FY 94 18% mod. 1030 4050 968 2582
FY 95 18% mod. 1025 3955 1018 3088
FY 96 18% mod. 1042 3903 1002 2845
weighted 1026 3993 990 2839 71
mean
FZ 23 10% add. 961 2872 880 1112
FZ 24 10% add. 980 3338 955 1253
FZ 25 10% add. 993 3056 1007 1577
FZ 26 10% add. 986 3070 969 1373
weighted 980 3155 953 1401 44
mean
FZ 33 14% add. 956 3337 980 1029
FZ 34 14% add. 983 3821 947 973
FZ 35 14% add. 987 3596 1015 1349
FZ 36 14% add. 873 2664 807 1240
weighted 950 3584 937 1206 34
FZ 43 18% add. 947 3463 968 1055
FZ 44 18% add. 962 3460 974 925
FZ 45 18% add. 994 4109 996 1076
FZ 46 18% add. 915 3298 955 838
Weighted 955 3677 973 1019 28
mean
______________________________________
TABLE 12
______________________________________
Internal bond strength - V313 cyclic testing
Board from 65% r.h. final
Ex Ref density IBS density
IBS retention
No. Type Kg/m.sup.3
kPa Kg/m.sup.3
kPa %
______________________________________
FZ 3 control 1008 1564 986 477
FZ 4 control 1005 1722 1022 451
FZ 5 control 1053 2353 1027 712
FZ 6 control 990 1855 985 69
weighted 1014 1977 1005 546 28
mean
FZ 12 10% mod. 1005 3677 953 1927
FZ 13 10% mod. 995 3573 990 2363
FZ 14 10% mod. 980 3733 948 2157
FZ 15 10% mod. 978 3620 991 2268
weighted 990 3677 971 2263 62
mean
FY 87 14% mod. 984 3143 940 2270
FY 88 14% mod. 996 3358 1015 2463
FY 89 14% mod. 1001 3431 1025 2649
FY 90 14% mod. 1044 3980 1037 2605
weighted 1006 3590 1004 2572 72
mean
FY 93 18% mod. 1008 3973 994 2711
FY 94 18% mod. 1030 4050 1007 2531
FY 95 18% mod. 1025 3955 1033 2356
FY 96 18% mod. 1042 3903 1006 2764
weighted 1026 3993 1010 2668 67
mean
FZ 23 10% add. 961 2872 980 1220
FZ 24 10% add. 980 3338 989 1326
FZ 25 10% add. 993 3056 932 518
FZ 26 10% add. 986 3070 1001 1489
weighted 980 3155 976 1345 43
mean
FZ 33 14% add. 956 3337 983 1167
FZ 34 14% add. 983 3821 1008 1003
FZ 35 14% add. 987 3596 1032 1196
FZ 36 14% add. 873 2664 896 1401
weighted 950 3584 980 1255 35
mean
FZ 43 18% add. 947 3463 970 1034
FZ 44 18% add. 962 3460 989 1409
FZ 45 18% add. 994 4109 1031 1129
FZ 46 18% add. 915 3298 966 1263
weighted 955 3677 989 1267 34
mean
______________________________________
TABLE 13
______________________________________
Internal bond strength - non-standard cyclic testing
Board from 65% r.h. final
Ex Ref density IBS density
IBS retention
No. Type Kg/m.sup.3
kPa Kg/m.sup.3
kPa %
______________________________________
FZ 3 control 1008 1564 975 485
FZ 4 control 1005 1722 1031 406
FZ 5 control 1053 2353 1004 413
FZ 6 control 990 1855 997 293
weighted 1014 1977 1001 435 22
mean
FZ 12 10% mod. 1005 3677 926 1263
FZ 13 10% mod. 995 3573 996 1556
FZ 14 10% mod. 980 3733 953 1520
FZ 15 10% mod. 978 3620 970 1470
weighted 990 3677 961 1515 41
mean
FY 87 14% mod. 984 3143 906 1259
FY 88 14% mod. 996 3358 1015 1423
FY 89 14% mod. 1001 3431 1029 1816
FY 90 14% mod. 1044 3980 1002 1645
weighted 1006 3590 988 1628 45
mean
FY 93 18% mod. 1008 3973 970 1380
FY 94 18% mod. 1030 4050 980 1454
FY 95 18% mod. 1025 3955 994 1899
FY 96 18% mod. 1042 3903 972 1662
weighted 1026 3993 979 1672 42
mean
FZ 23 10% add. 961 2872 959 771
FZ 24 10% add. 980 3338 998 944
FZ 25 10% add. 993 3056 919 763
FZ 26 10% add. 986 3070 1002 1020
weighted 980 3155 969 912 29
mean
FZ 33 14% add. 956 3337 984 746
FZ 34 14% add. 983 3821 1018 726
FZ 35 14% add. 987 3596 1030 747
FZ 36 14% add. 873 2664 925 1115
weighted 950 3584 989 869 24
mean
FZ 43 18% add. 947 3463 987 680
FZ 44 18% add. 962 3460 961 702
FZ 45 18% add. 994 4109 1054 684
FZ 46 18% add. 915 3298 1006 618
weighted 955 3677 1002 689 19
mean
______________________________________
TABLE 14
______________________________________
Thickness swell and linear expansion from
manufacture to 65% r.h.
Board from Thickness Linear
Ex Ref swell expansion
No. Type % %
______________________________________
FZ 3 control 3 0.2
FZ 4 control 3 0.0
FZ 5 control 3 0.2
FZ 6 control 3 0.2
mean 2.9 0.16
FZ 12 10% mod. 3 0.4
FZ 13 10% mod. 2 0.3
FZ 14 10% mod. 3 0.3
FZ 15 10% mod. 3 0.3
mean 2.6 0.34
FY 87 14% mod.
FY 88 14% mod. 0.4
FY 89 14% mod. 2 0.3
FY 90 14% mod. 3 0.4
mean 2.4 0.35
FY 93 18% mod.
FY 94 18% mod. 2 0.2
FY 95 18% mod. 1 0.3
FY 96 18% mod. 1 -0.0
mean 1.6 0.17
FX 23 10% add. 2 0.0
FZ 24 10% add. 1 0.0
FZ 25 10% add. 0 0.1
FZ 26 10% add. -0 0.0
mean 0.8 0.03
FZ 33 14% add. 0 0.2
FZ 34 14% add. 0 0.1
FZ 35 14% add. 0 0.0
FZ 36 14% add. 0 0.1
mean 0.3 0.12
FZ 43 18% add. -0 0.1
FZ 44 18% add. -0 0.1
FZ 45 18% add. -1 0.1
FZ 46 18% add. -0 0.2
mean -0.3 0.13
______________________________________
TABLE 15
______________________________________
Weight gain, thickness swell and linear expansion from
65% r.h. to 93% r.h.
Board from Weight Thickness
Linear
Ex Ref gain swell expansion
No. Type % % %
______________________________________
FZ 3 control 5.5 6.1 0.10
FZ 4 control 3.5 3.6 -0.10
FZ 5 control 4.7 5.2 0.15
FZ 6 control 4.3 4.9 0.00
mean 4.5 5.0 0.04
FZ 12 10% mod. 3.3 3.5 0.15
FZ 13 10% mod. 4.3 4.4 0.15
FZ 14 10% mod. 3.7 3.4 -0.05
FZ 15 10% mod. 3.7 3.2 -0.10
mean 3.7 3.6 0.04
FY 87 14% mod. 3.8 3.1 0.05
FY 88 14% mod. 2.9 2.5 -0.25
FY 89 14% mod. 3.7 3.0 0.00
FY 90 14% mod. 3.6 3.0 0.20
mean 3.5 2.9 0.00
FY 93 18% mod. 3.0 2.3 -0.10
FY 94 18% mod. 2.4 1.6 -0.10
FY 95 18% mod. 3.8 2.9 -0.05
FY 96 18% mod. 2.5 2.0 0.05
mean 2.9 2.2 -0.05
FZ 23 10% add. 4.9 3.8 0.25
FZ 24 10% add. 5.1 3.9 0.40
FZ 25 10% add. 6.0 5.1 0.30
FZ 26 10% add. 5.0 3.8 0.25
mean 5.3 4.1 0.30
FZ 33 14% add. 5.5 4.6 0.40
FZ 34 14% add. 4.6 3.6 0.25
FZ 35 14% add. 4.0 4.0 0.30
FZ 36 14% add. 4.7 3.4 0.30
mean 4.7 3.9 0.31
FZ 43 18% add. 5.3 4.6 0.25
FZ 44 18% add. 5.2 4.0 0.20
FZ 45 18% add. 5.0 3.6 0.40
FZ 46 18% add. 5.3 4.3 0.40
mean 5.2 4.1 0.31
______________________________________
TABLE 16
______________________________________
Weight gain, thickness swell and linear expansion from 65% r.h.
to 1 hour 20.degree. C. soak
Board from Weight
Thickness
Linear
Ex Ref density gain swell expansion
No. Type Kg/m.sup.3
% % %
______________________________________
FZ 3 control 987 4.8 3.3 0.35
FZ 4 control 1034 4.4 3.3 -0.10
FZ 5 control 1031 4.2 3.4 -0.05
FZ 6 control 1027 4.5 3.5 0.15
mean 1020 4.5 3.3 0.09
FZ 12 10% mod. 967 3.7 2.3 0.15
FZ 13 10% mod. 1005 2.7 1.9 -0.05
FZ 14 10% mod. 959 3.7 1.9 0.10
mean 977 3.3 2.0 0.07
FY 87 14% mod. 965 2.1 1.0 0.05
FY 88 14% mod. 980 1.6 0.9 0.00
FY 89 14% mod. 972 2.5 1.4 -0.05
FY 90 14% mod. 998 2.0 1.1 -0.05
mean 979 2.1 1.1 -0.01
FY 93 18% mod. 966 1.4 0.5 0.00
FY 94 18% mod. 999 1.7 0.6 -0.05
FY 95 18% mod. 1003 1.5 0.7 -0.10
FY 96 18% mod. 1024 1.5 0.9 0.00
mean 998 1.5 0.7 -0.04
FZ 23 10% add. 971 1.9 0.8 -0.10
FZ 24 10% add. 973 2.3 0.8 -0.15
FZ 25 10% add. 973 4.6 1.4 -0.05
FZ 26 10% add. 1013 2.2 1.2 -0.15
mean 983 2.7 1.1 -0.11
FZ 33 14% add. 1039 1.1 0.4 0.15
FZ 34 14% add. 993 2.1 0.9 -0.30
FZ 35 14% add. 1014 1.5 0.5 0.25
FZ 36 14% add. 976 1.9 0.7 -0.05
mean 1006 1.7 0.6 0.01
FZ 43 18% add. 989 1.0 0.5 -0.35
FZ 44 18% add. 998 1.6 0.2 0.15
FZ 45 18% add. 1033 1.7 0.4 -0.10
FZ 46 18% add. 1012 1.1 0.4 0.00
mean 1008 1.3 0.4 -0.07
______________________________________
TABLE 17
______________________________________
Weight gain, thickness smell and linear expansion from
65% r.h. to 42 hour 20.degree. C. soak
Board from Weight
Thickness
Linear
Ex Ref density gain swell expansion
No. Type Kg/m.sup.3
% % %
______________________________________
FZ 3 control 987 22.6 8.7 0.25
FZ 4 control 1034 20.1 9.4 0.30
FZ 5 control 1031 23.6 9.5 0.30
FZ 6 control 1027 21.6 10.4 0.45
mean 1020 22.0 9.5 0.32
FZ 12 10% mod. 967 15.4 4.3 0.30
FZ 13 10% mod. 1005 11.9 5.6 -0.05
FZ 14 10% mod. 959 15.1 5.1 0.00
mean 977 14.1 5.0 0.08
FY 87 14% mod. 965 10.1 3.0 0.00
FY 88 14% mod. 980 7.6 2.8 0.10
FY 89 14% mod. 972 11.2 3.9 0.05
FY 90 14% mod. 998 9.5 3.4 0.15
mean 979 9.6 3.3 0.07
FY 93 18% mod. 966 6.9 2.5 0.25
FY 94 18% mod. 999 7.3 2.4 0.10
FY 95 18% mod. 1003 6.2 2.2 0.15
FY 96 18% mod. 1024 6.7 2.7 0.00
mean 998 6.8 2.5 0.12
FZ 23 10% add. 971 12.7 4.8 0.05
FZ 24 10% add. 973 12.6 4.5 0.10
FZ 25 10% add. 973 15.6 6.9 0.10
FZ 26 10% add. 1013 9.7 4.6 0.10
mean 983 12.7 5.2 0.09
FZ 33 14% add. 1039 8.1 4.7 0.05
FZ 34 14% add. 993 10.9 4.7 -0.05
FZ 35 14% add. 1014 8.9 4.5 0.20
FZ 36 14% add. 976 11.7 4.4 0.25
mean 1006 9.9 4.6 0.11
FZ 43 18% add. 989 8.2 4.2 0.05
FZ 44 18% add. 998 10.6 4.5 0.25
FZ 45 18% add. 1033 8.4 3.9 0.10
FZ 46 18% add. 1012 7.2 3.8 0.10
mean 1008 8.6 4.1 0.12
______________________________________
TABLE 18
______________________________________
Weight gain, thickness swell and linear expansion from
65% r.h. to 2 hour boil
Board from Weight Thickness
Linear
Ex Ref gain swell expansion
No. Type % % %
______________________________________
FZ 3 control 83.4 48.4 0.65
FZ 4 control 98.7 65.0 1.05
FZ 5 control 89.0 54.7 1.25
FZ 6 control 101.8 62.7 0.95
mean 93.2 57.7 0.97
FZ 12 10% mod. 60.9 21.4 0.35
FZ 13 10% mod. 52.2 20.7 0.20
FZ 14 10% mod. 54.5 18.5 0.25
FZ 15 10% mod. 53.5 18.3 0.30
mean 55.3 19.8 0.27
FY 87 14% mod. 51.6 16.3 0.20
FY 88 14% mod. 40.7 14.7 -0.05
FY 89 14% mod. 41.5 16.1 0.30
FY 90 14% mod. 44.3 15.5 0.35
mean 44.5 15.6 0.20
FY 93 18% mod. 42.7 13.0 0.20
FY 94 18% mod. 42.9 13.3 0.40
FY 95 18% mod. 39.9 14.0 0.20
FY 96 18% mod. 45.4 14.7 0.50
mean 42.7 13.8 0.32
FZ 23 10% add. 51.2 18.8 0.30
FZ 24 10% add. 43.4 19.6 0.40
FZ 25 10% add. 42.8 19.1 0.30
FZ 26 10% add. 45.8 19.7 0.30
mean 45.8 19.3 0.32
FZ 33 14% add. 44.8 20.6 0.35
FZ 34 14% add. 39.8 19.9 0.45
FZ 35 14% add. 40.6 18.2 0.40
FZ 36 14% add. 50.7 17.2 0.40
mean 44.0 19.0 0.40
FZ 43 18% add. 45.2 20.0 0.35
FZ 44 18% add. 47.3 17.5 0.45
FZ 45 18% add. 35.2 16.9 0.40
FZ 46 18% add. 42.5 20.5 0.45
mean 42.6 18.7 0.41
______________________________________
TABLE 19
______________________________________
Expansion and weight gain - V313 cyclical testing
Board from Weight
Thickness
Linear
Ex Ref density gain swell expansion
No. Type Kg/m.sup.3
% % %
______________________________________
FZ 3 control 986 17.7 0.08 0.90
FZ 4 control 1022 20.9 0.14 0.81
FZ 5 control 1027 13.1 0.11 0.89
FZ 6 control 985 26.5 0.18 0.56
mean 1005 19.6 0.13 0.79
FZ 12 10% mod. 953 8.8 -0.15 0.07
FZ 13 10% mod. 990 5.2 -0.08 0.26
FZ 14 10% mod. 948 5.8 -0.11 0.04
FZ 15 10% mod. 991 4.5 -0.11 0.37
mean 971 6.1 -0.11 0.18
FY 87 14% mod. 940 3.7 -0.08 -0.04
FY 88 14% mod. 1015 1.9 -0.10 0.00
FY 89 14% mod. 1025 3.4 -0.13 -0.07
FY 90 14% mod. 1037 2.0 -0.15 -0.36
mean 1004 2.8 -0.12 -0.12
FY 93 18% mod. 994 2.0 -0.10 -0.33
FY 94 18% mod. 1007 2.3 -0.09 -0.22
FY 95 18% mod. 1033 1.8 -0.14 -0.51
FY 96 18% mod. 1006 1.9 -0.10 -0.53
mean 1010 2.0 -0.11 -0.39
FZ 23 10% add. 980 6.5 -0.17 0.34
FZ 24 10% add. 989 4.9 -0.25 0.07
FZ 25 10% add. 932 6.6 -0.13 -1.33
FZ 26 10% add. 1001 3.8 -0.17 -0.56
mean 976 5.4 -0.18 -0.37
FZ 33 14% add. 983 4.8 -0.22 0.11
FZ 34 14% add. 1008 6.7 -0.32 -0.38
FZ 35 14% add. 1032 4.2 -0.29 -0.96
FZ 36 14% add. 896 4.7 -0.19 -0.41
mean 980 5.1 -0.26 -0.41
FZ 43 18% add. 970 4.3 -0.17 -0.35
FZ 44 18% add. 989 4.0 -0.20 -0.30
FZ 45 18% add. 1031 4.2 -0.35 -1.70
FZ 46 18% add. 966 5.3 -0.22 -0.76
mean 989 4.5 -0.24 -0.78
______________________________________
TABLE 20
______________________________________
Expansion and weight gain - non-standard cyclic testi
Board from Weight
Thickness
Linear
Ex Ref density gain swell expansion
No. Type Kg/m.sup.3
% % %
______________________________________
FZ 3 control 975 15.8 0.11 5.4
FZ 4 control 1031 20.5 0.12 4.7
FZ 5 control 1004 20.5 0.03 4.9
FZ 6 control 997 23.1 0.22 4.6
mean 1001 20.0 0.12 4.9
FZ 12 10% mod. 926 5.0 -0.33 8.0
FZ 13 10% mod. 996 5.2 -0.39 6.6
FZ 14 10% mod. 953 4.2 -0.47 7.5
FZ 15 10% mod. 970 4.9 -0.55 6.8
mean 961 4.8 -0.44 7.2
FY 87 14% mod. 906 2.9 -0.57 9.2
FY 88 14% mod. 1015 1.1 -0.58 6.7
FY 89 14% mod. 1029 2.9 -0.63 7.0
FY 90 14% mod. 1002 0.9 -0.72 7.7
mean 988 1.9 -0.63 7.7
FY 93 18% mod. 970 -0.6 -0.68 9.0
FY 94 18% mod. 980 1.1 -0.71 8.4
FY 95 18% mod. 994 -0.6 -0.64 7.9
FY 96 18% mod. 972 0.9 -0.55 8.7
mean 979 0.2 -0.65 8.5
FZ 23 10% add. 959 4.1 -0.58 7.2
FZ 24 10% add. 998 3.1 -0.52 6.3
FZ 25 10% add. 919 2.1 -0.60 9.0
FZ 26 10% add. 1002 3.0 -0.57 6.7
mean 969 3.1 -0.57 7.3
FZ 33 14% add. 984 3.3 -0.72 7.4
FZ 34 14% add. 1018 2.3 -0.52 7.5
FZ 35 14% add. 1030 2.6 -0.52 7.8
FZ 36 14% add. 925 0.5 -0.70 8.9
mean 989 2.2 -0.62 7.9
FZ 43 18% add. 987 2.2 -0.54 9.3
FZ 44 18% add. 961 0.7 -0.67 9.9
FZ 45 18% add. 1054 0.5 -0.60 10.6
FZ 46 18% add. 1006 1.3 -0.70 8.8
mean 1002 1.2 -0.63 9.7
______________________________________
TABLE 21
______________________________________
Oven dry thickness swell - non-standard cyclic testing
Board from cycle
cycle
cycle
cycle
cycle
Ex Ref density 1 2 3 4 5
No. Type Kg/m.sup.3
% % % % %
______________________________________
FZ 3 control 975 10.3 13.5 15.1 15.7 15.3
FZ 4 control 1031 13.6 17.4 18.5 19.5 19.9
FZ 5 control 1004 10.5 14.8 16.2 16.6 16.3
FZ 6 control 997 15.5 18.1 20.6 22.7 22.1
mean 1001 12.5 15.9 17.6 18.6 18.4
FZ 12 10% mod. 926 6.1 6.3 5.8 5.2 5.3
FZ 13 10% mod. 996 4.8 5.4 5.3 4.7 5.6
FZ 14 10% mod. 953 5.1 5.6 5.6 4.9 4.7
FZ 15 10% mod. 970 4.5 4.1 5.6 5.5 5.3
mean 961 5.1 5.3 5.6 5.1 5.2
FY 87 14% mod. 906 3.3 3.0 2.1 1.8 1.5
FY 88 14% mod. 1015 2.1 1.9 1.6 1.8 1.4
FY 89 14% mod. 1029 3.6 3.6 3.7 3.2 3.7
FY 90 14% mod. 1002 2.5 2.4 1.8 1.8 1.9
mean 988 2.9 2.7 2.3 2.2 2.1
FY 93 18% mod. 970 0.6 0.7 0.7 0.5 0.1
FY 94 18% mod. 980 0.9 1.1 0.7 1.2 1.8
FY 95 18% mod. 994 1.2 1.6 1.0 1.4 0.6
FY 96 18% mod. 972 0.8 1.5 1.4 0.3 0.6
mean 979 0.9 1.2 1.0 0.8 0.8
FZ 23 10% add. 959 1.8 2.8 3.7 3.1 3.8
FZ 24 10% add. 998 4.2 4.2 5.0 3.7 3.7
FZ 25 10% add. 919 2.6 3.1 3.7 3.4 2.9
FZ 26 10% add. 1002 2.4 3.2 3.5 3.6 3.1
mean 969 2.7 3.3 4.0 3.4 3.4
FZ 33 14% add. 984 2.5 3.0 2.4 2.5 3.4
FZ 34 14% add. 1018 1.3 1.7 2.0 1.4 2.4
FZ 35 14% add. 1030 2.6 2.2 2.0 2.9 3.0
FZ 36 14% add. 925 0.9 2.4 0.8 1.2 0.8
mean 989 1.9 2.3 1.8 2.0 2.4
FZ 43 18% add. 987 2.4 2.8 2.5 2.8 2.3
FZ 44 18% add. 961 1.3 2.4 1.7 1.1 0.9
FZ 45 18% add. 1054 1.1 2.3 2.3 2.6 1.6
FZ 46 18% add. 1006 1.8 2.3 1.9 2.1 1.8
mean 1002 1.6 2.4 2.1 2.2 1.6
______________________________________
TABLE 22
______________________________________
Oven dry weight loss - non-standard cyclic testing
Board from cycle
cycle
cycle
cycle
cycle
Ex Ref density 1 2 3 4 5
No. Type Kg/u.m. % % % % %
______________________________________
FZ 3 control 975 1.1 2.1 3.4 4.7 5.9
FZ 4 control 1031 0.9 1.9 3.0 3.8 4.6
FZ 5 control 1004 0,9 1.9 3.0 3.9 5.4
FZ 6 control 997 1.0 2.1 3.2 4.1 5.2
mean 1001 1.0 2.0 3.1 4.1 5.3
FZ 12 10% mod. 926 1.8 3.4 5.3 6.7 8.0
FZ 13 10% mod. 996 1.5 2.9 4.5 5.6 6.4
FZ 14 10% mod. 953 1.6 3.1 5.1 6.3 7.4
FZ 15 10% mod. 970 1.5 3.0 4.6 5.7 6.9
mean 961 1.6 3.1 4.9 6.1 7.2
FY 87 14% mod. 906 1.8 3.6 5.8 7.3 8.9
FY 88 14% mod. 1015 1.4 2.7 4.4 5.3 6.2
FY 89 14% mod. 1029 1.6 2.9 4.7 5.6 6.6
FY 90 14% mod. 1002 1.7 3.3 4.9 6.2 7.3
mean 988 1.6 3.1 4.9 6.1 7.2
FY 93 18% mod. 970 1.7 3.5 5.7 7.0 8.1
FY 94 18% mod. 980 1.6 3.4 5.4 6.5 7.7
FY 95 18% mod. 994 1.8 3.3 5.2 6.3 7.3
FY 96 18% mod. 972 1.8 3.5 5.6 6.7 7.9
mean 979 1.7 3.4 5.5 6.6 7.7
FZ 23 10% add. 959 1.8 3.2 4.9 6.1 7.3
FZ 24 10% add. 998 1.4 2.7 4.3 5.2 6.1
FZ 25 10% add. 919 1.8 3.9 5.8 7.3 8.6
FZ 26 10% add. 1002 1.5 2.8 4.4 5.4 6.5
mean 969 1.6 3.2 4.8 6.0 7.2
FZ 33 14% add. 984 1.7 3.3 5.1 6.3 7.4
FZ 34 14% add. 1018 1.6 3.0 4.8 6.0 7.0
FZ 35 14% add. 1030 1.8 3.4 5.2 6.3 7.3
FZ 36 14% add. 925 1.9 3.6 5.6 7.3 8.7
mean 989 1.7 3.3 5.2 6.5 7.6
FZ 43 18% add. 987 2.2 4.0 6.1 7.4 9.1
FZ 44 18% add. 961 1.8 4.4 6.5 8.0 9.2
FZ 45 18% add. 1054 2.2 4.0 6.0 7.6 9.0
FZ 46 18% add. 1006 1.9 3.7 5.8 7.1 8.1
mean 1002 2.0 4.0 6.1 7.5 8.9
______________________________________
The above results show that the treatment of lignocellulosic materials according to the present invention improves the boards produced therefrom in respect of:
i. Static Bending:
Both strength and stiffness when dry or wet;
Toughness when wet; and
Retention of physical properties when wet.
ii. Internal Bond Strength:
Dry bond strength
iii. Initial Swell:
Reducing thickness swell
Reducing linear expansion
iv. Linear Expansion:
Reducing linear expansion upon soaking
v. Thickness Swell:
Reducing thickness swell due to simulated weathering and cold water soaking.
vi. Water Uptake:
Reducing water uptake due either to cold soak or boiling or to high humidity
vii. Cyclical Testing:
Reducing thickness swell during cyclical boiling.
Claims
1. A process for modifying lignocellulosic material by a chemical treatment method, said method comprising treating the lignocellulosic material with:
- a. phthalic anhydride and
- b. a thermosetting resin selected from consisting of phenol-formaldehyde resins; urea formaldehyde resins and urethane resins, and hat curing the phthalylated resin-impregnated product so formed.
2. A process according to claim 1 wherein the lignocellulosic material is a form of wood selected from the group consisting of chips, flakes, splinters, strands, shreds, shives and fibres.
3. A process according to claim 1 wherein each of phthalic anhydride and the thermosetting resin are in the same or different form of a powdered solid, or, a solution or a dispersion in the same solvent or different compatible solvents.
4. A process according to claim 1 wherein the phthalic anhydride used for treating the lignocellulosic material is in the solid form.
5. A process according to claim 1 wherein the amount of phthalic anhydride used is 1 to 50% by weight of the lignocellulosic material.
6. A process as claimed in claim 1, wherein the lignocellulosic material is treated sequentially with said phthalic anhydride and said thermosetting resin.
7. A process as claimed in claim 1, wherein the lignocellulosic material is treated simultaneously with said phthalic anhydride and said thermosetting resin.
8. A process according to any one of the preceding claims wherein the lignocellulosic material is sequentially treated by bringing the material into contact with phthalic anhydride at elevated temperature and the phthalylated material so formed is impregnated with a thermosetting resin.
9. A process according to claim 7 wherein the lignocellulosic material is treated with phthalic anhydride by a cooking process carried out at a temperature of at least 100.degree. C.
10. A process according to claim 7 wherein the lignocellulosic material is treated with phthalic anhydride until the treated material has acquired a weight gain of at least 15%.
11. A process according to claim 7 wherein the phthalylated lignocellulosic material is dampened with water prior to impregnation thereof with a thermosetting resin in its powder form.
12. A process according to claim 7 wherein the heat curing of the phthalylated, resin-impregnated lignocellulosic material is carried out at a temperature in the range from 150.degree. to 250.degree. C.
13. A process according to claim 7 wherein the heat curing step of the phthalylated, resin-impregnated lignocellulosic material in fibrous or particulate or shredded form is carried out by pressing in a die with a pre-heated punch to 5.5 ml stops at a temperature of 180.degree. C. to produce a shaped or moulded product.
14. A process according to claim 7 wherein the lignocellulosic material is pre-dried to a constant weight prior to treatment with phthalic anhydride.
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- Rowell, R et al, "The Chemistry of Solid Wood", American Chemical Society, (1984) pp. 186 and 208. Popper et al, Holz Roh Werkst (1972) 30 (8), pp. 289-294; (1973), 31 (2), pp. 65-70; and (1975) 33(11). pp. 415-419.
Type: Grant
Filed: Sep 17, 1993
Date of Patent: Jan 31, 1995
Assignee: BP Chemicals Limited (London)
Inventors: Harold A. Earl (Clwyd), Richard J. Salisbury (Gwynedd)
Primary Examiner: Michael Lusignan
Law Firm: Brooks Haidt Haffner & Delahunty
Application Number: 8/123,534
International Classification: B05D 700;
